固相微萃取-气相色谱-负化学源质谱法测定葡萄酒中2,4,6-三氯苯甲醚

目的建立葡萄酒中2,4,6-三氯苯甲醚(2,4,6-TCA)的固相微萃取-气相色谱-负化学源电离的质谱联用法(SPME-NCI-GC/MS)。方法在35℃下,采用100μm聚二甲基硅氧烷共聚物(PDMS)的固相微萃取纤维对葡萄酒样品萃取15min,在气相色谱仪的进样口解析后,经毛细管柱CP-SIL 8CB-MS(30m×0.25mm×0.25μm)分离,负化学离子源电离的质谱法测定,采用选择离子监测方式(SIM)进行监测,以d5-2,4,6-TCA为内标,进行内标法定量。结果在0.5～60ng/L范围内,葡萄酒样品中的2,4,6-TCA含量与2,4,6-TCA及内标d5-2,4,6-TCA峰面积比呈良好的线性关系,r>0.996。以空白葡萄酒基质进行加标回收实验,3个添加水平(5、10和20ng/L)的回收率为79.8%～101.6%,RSD≤7%(n=5)。葡萄酒中2,4,6-TCA的检测限和定量限分别为0.06和0.2ng/L。结论该方法无需使用有机溶剂,选择性好,灵敏度高,适用于葡萄酒中痕量2,4,6-TCA的测定。

Determination of 2,4,6-trichloroanisole in wine by head-space solid phase micro-extraction and gas chromatography-mass spectrometry

Objective To establish a method of combining gas chromatography-mass spectrometry(GC-MS) with head-space solid phase micro-extraction(HS-SPME) for the detection of 2,4,6-trichloroanisole(2,4,6-TCA) in wine.Methods 2,4,6-TCA in wine were extracted by polydimethylsiloxane(PDMS,100μm)fiber for 15 min under 35℃ in a water bath.The fiber was then transferred into the injection port of the GC-MS and separated by a CP-SIL 8CB-MS capillary column(30m×0.25mm×0.25μm),and detected by mass spectrometry using d5-2,4,6-TCA as an internal standard.Results The linear range for 2,4,6-TCA was 5(60ng/L,the detection limit was 0.06ng/L.The recovery of standard addition(5,10,20ng/L) was in the range of 79.8%(101.6% with relative standard deviations(RSD,n=5)≤7%.Conclusion Organic solvents were avoided and the selection was sensitive for the method,which is suitable for the determination of 2,4,6-TCA in wine.